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从层状双氢氧化物到尖晶石纳米结构:纳米片和纳米棒的简便合成与表征

From layered double hydroxide to spinel nanostructures: facile synthesis and characterization of nanoplatelets and nanorods.

作者信息

Sun Genban, Sun Lingna, Wen He, Jia Zhiqian, Huang Kunlin, Hu Changwen

机构信息

The Institute for Chemical Physics and Department of Chemistry, Beijing Institute of Technology, Beijing 100081, P.R. China.

出版信息

J Phys Chem B. 2006 Jul 13;110(27):13375-80. doi: 10.1021/jp060916d.

DOI:10.1021/jp060916d
PMID:16821857
Abstract

Mg-Al spinel (MgAl2O4) nanorods and nanoplatelets transformed from Mg-Al layered double hydroxide (Mg-Al-LDHs) were synthesized via a combined hydrothermal method and calcination route using Al(NO3).9H2O and Mg(NO3)2.6H2O as raw materials. The nanorods and nanoplatelets were characterized by means of physical techniques, including powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microcopy (HRTEM), selected-area electron diffraction (SAED), Fourier transform infrared spectra (FT-IR), thermogravimetric (TG), and nitrogen adsorption-desorption isotherms. XRD patterns reveal that the Mg-Al-LDHs nanostructures were obtained under a hydrothermal reaction temperature of 200 degrees C and Mg-Al spinel nanostructures were fabricated via calcination of the Mg-Al-LDHs nanostructures at 750 degrees C. It can be seen from TEM that the sizes of the Mg-Al-LDHs nanoplatelets were about 20-40 nm and the diameters of the MgAl2O4 nanorods were ca. 6 nm. The HRTEM images indicate that the crystal lattice spaces of the MgAl2O4 nanorods and nanoplatelets are 0.282 and 0.287 nm, respectively.

摘要

以硝酸铝九水合物(Al(NO₃)·9H₂O)和硝酸镁六水合物(Mg(NO₃)₂·6H₂O)为原料,采用水热法和煅烧相结合的路线,合成了由镁铝层状双氢氧化物(Mg-Al-LDHs)转变而来的镁铝尖晶石(MgAl₂O₄)纳米棒和纳米片。通过粉末X射线衍射(XRD)、透射电子显微镜(TEM)、高分辨率透射电子显微镜(HRTEM)、选区电子衍射(SAED)、傅里叶变换红外光谱(FT-IR)、热重分析(TG)和氮吸附-脱附等温线等物理技术对纳米棒和纳米片进行了表征。XRD图谱表明,在200℃的水热反应温度下获得了Mg-Al-LDHs纳米结构,通过在750℃煅烧Mg-Al-LDHs纳米结构制备了镁铝尖晶石纳米结构。从TEM可以看出,Mg-Al-LDHs纳米片的尺寸约为20-40nm,MgAl₂O₄纳米棒的直径约为6nm。HRTEM图像表明,MgAl₂O₄纳米棒和纳米片的晶格间距分别为0.282和0.287nm。

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